Reaktion #618396

Reaktionsgleichung

CH2Cl2

abiraterone

methanol

→

DHEA

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperatur(reflux)
2. 2
   SonstigeThe CH2Cl2 was then removed by distillation at atmospheric pressure
3. 3
   TemperaturThe mixture was cooled to 0-5° C.
4. 4
   Temperaturmaintained 1 hour at 0-5° C
5. 5
   FiltrationThe suspension was filtered
6. 6
   Filtration(fast filtration)
7. 7
   Waschenthe cake was washed twice with 4.4 ml of methanol
8. 8
   Temperaturcooled to 0-5° C
9. 9
   SonstigeThe wet solid was dried at 40-45° C. under vacuum for 5 hours
10. 10
    Sonstigeto give
11. 11
    Sonstige7.2 g (yield of purification 82.8%) of pure stage 3 (abiraterone)

Vorschrift

34.8 ml of CH2Cl2 and 26.1 ml of methanol were added to 8.7 g (24.9 mmol) of crude stage 3 (abiraterone). The mixture was heated to 40-45° C. (reflux), to have a solution. The CH2Cl2 was then removed by distillation at atmospheric pressure. The mixture was cooled to 0-5° C., and then maintained 1 hour at 0-5° C. The suspension was filtered (fast filtration) and the cake was washed twice with 4.4 ml of methanol cooled to 0-5° C. The wet solid was dried at 40-45° C. under vacuum for 5 hours to give 7.2 g (yield of purification 82.8%) of pure stage 3 (abiraterone). The overall yield from DHEA was around 50%.

Quelle